#------------------------------------------------------------------------------ #$Date: 2026-06-04 17:58:32 +0100 (Thu, 04 Jun 2026) $ #$Revision: 306210 $ #$URL: svn://www.crystallography.net/cod/cif/7/72/10/7721078.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_7721078 loop_ _publ_author_name 'Kong, Yin-Cong' 'Yang, Zi' 'Liu, Yi' 'Wang, Chen' 'Sun, Rong' 'Sun, Zheng' 'Wang, Bing-Wu' 'Gao, Song' _publ_section_title ; A dysprosium alkylidene single molecule magnet. ; _journal_issue 19 _journal_name_full 'Dalton transactions (Cambridge, England : 2003)' _journal_page_first 7492 _journal_page_last 7496 _journal_paper_doi 10.1039/d6dt00641h _journal_volume 55 _journal_year 2026 _chemical_formula_moiety 'C25 H42 Cl2 Dy N3 O' _chemical_formula_sum 'C25 H42 Cl2 Dy N3 O' _chemical_formula_weight 634.01 _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_Hall '-P 1' _space_group_name_H-M_alt 'P -1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary iterative _audit_creation_date 2025-02-22 _audit_creation_method ; Olex2 1.5 (compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817) ; _audit_update_record ; 2026-01-22 deposited with the CCDC. 2026-04-20 downloaded from the CCDC. ; _cell_angle_alpha 75.400(2) _cell_angle_beta 73.024(2) _cell_angle_gamma 75.3690(10) _cell_formula_units_Z 2 _cell_length_a 10.3923(4) _cell_length_b 10.9758(4) _cell_length_c 13.5542(5) _cell_measurement_reflns_used 9877 _cell_measurement_temperature 200.00 _cell_measurement_theta_max 72.43 _cell_measurement_theta_min 3.02 _cell_volume 1403.92(9) _computing_cell_refinement 'SAINT V8.40B (?, 2016)' _computing_data_reduction 'SAINT V8.40B (?, 2016)' _computing_molecular_graphics 'Olex2 1.5 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 1.5 (Dolomanov et al., 2009)' _computing_structure_refinement 'SHELXL 2018/3 (Sheldrick, 2015)' _computing_structure_solution 'olex2.solve 1.5 (Bourhis et al., 2015)' _diffrn_ambient_temperature 200.00 _diffrn_measured_fraction_theta_full 0.987 _diffrn_measured_fraction_theta_max 0.988 _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_type GaK\a _diffrn_radiation_wavelength 1.34138 _diffrn_reflns_av_R_equivalents 0.0905 _diffrn_reflns_av_unetI/netI 0.0607 _diffrn_reflns_Laue_measured_fraction_full 0.987 _diffrn_reflns_Laue_measured_fraction_max 0.988 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_number 28925 _diffrn_reflns_point_group_measured_fraction_full 0.987 _diffrn_reflns_point_group_measured_fraction_max 0.988 _diffrn_reflns_theta_full 53.594 _diffrn_reflns_theta_max 54.998 _diffrn_reflns_theta_min 3.022 _exptl_absorpt_coefficient_mu 15.035 _exptl_absorpt_correction_T_max 0.7536 _exptl_absorpt_correction_T_min 0.2300 _exptl_absorpt_correction_type none _exptl_absorpt_process_details ; SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1764 before and 0.0895 after correction. The Ratio of minimum to maximum transmission is 0.3052. The \l/2 correction factor is Not present. ; _exptl_crystal_colour yellow _exptl_crystal_colour_primary yellow _exptl_crystal_density_diffrn 1.500 _exptl_crystal_description block _exptl_crystal_F_000 642 _exptl_crystal_size_max 0.13 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.11 _refine_diff_density_max 1.701 _refine_diff_density_min -1.870 _refine_diff_density_rms 0.136 _refine_ls_extinction_coef 0.0107(7) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method 'SHELXL-2018/3 (Sheldrick 2018)' _refine_ls_goodness_of_fit_ref 1.080 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 298 _refine_ls_number_reflns 5300 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.080 _refine_ls_R_factor_all 0.0460 _refine_ls_R_factor_gt 0.0430 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0734P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1109 _refine_ls_wR_factor_ref 0.1142 _reflns_Friedel_coverage 0.000 _reflns_number_gt 4876 _reflns_number_total 5300 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d6dt00641h2.cif _cod_data_source_block 230608d_0m _cod_database_code 7721078 _shelx_shelxl_version_number 2018/3 _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _shelx_estimated_absorpt_t_max 0.289 _shelx_estimated_absorpt_t_min 0.245 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups At 1.5 times of: All C(H,H,H) groups 2.a Ternary CH refined with riding coordinates: C7(H7), C10(H10) 2.b Secondary CH2 refined with riding coordinates: C18(H18a,H18b), C19(H19a,H19b), C25(H25a,H25b), C24(H24a,H24b), C23(H23a, H23b), C22(H22a,H22b) 2.c Aromatic/amide H refined with riding coordinates: C15(H15), C5(H5), C4(H4), C3(H3) 2.d Idealised Me refined as rotating group: C17(H17a,H17b,H17c), C13(H13a,H13b,H13c), C21(H21a,H21b,H21c), C20(H20a,H20b, H20c), C8(H8a,H8b,H8c), C9(H9a,H9b,H9c), C12(H12a,H12b,H12c), C11(H11a,H11b, H11c) ; _shelx_res_file ; TITL 230608d_0m_a.res in P-1 230608d_0m.res created by SHELXL-2018/3 at 14:25:28 on 22-Feb-2025 REM Old TITL 230608d_0m in P-1 #2 REM SHELXT solution in P-1: R1 0.096, Rweak 0.018, Alpha 0.033 REM 0.000 for 0 systematic absences, Orientation as input REM Formula found by SHELXT: C11 Cl2 Dy N6 O2 CELL 1.34138 10.3923 10.9758 13.5542 75.4 73.024 75.369 ZERR 2 0.0004 0.0004 0.0005 0.002 0.002 0.001 LATT 1 SFAC C H Cl Dy N O DISP C 0.0137 0.0067 57.1 DISP Cl 0.3281 0.5435 4162.2 DISP Dy -5.9987 12.4498 95237.5 DISP H -0 0 0.6481 DISP N 0.0241 0.0134 109.9 DISP O 0.0389 0.0241 193.4 UNIT 50 84 4 2 6 2 L.S. 4 PLAN 11 SIZE 0.11 0.13 0.12 TEMP -73.15 CONF BOND list 4 MORE -1 BOND $H fmap 2 acta OMIT -2 110 OMIT 1 1 0 OMIT 1 4 1 OMIT 3 1 0 REM REM REM WGHT 0.073400 EXTI 0.010655 FVAR 0.75216 DY1 4 0.720231 0.364568 0.715792 11.00000 0.03091 0.02325 = 0.02004 -0.00422 -0.00557 -0.01060 CL1 3 0.984548 0.315281 0.651012 11.00000 0.03266 0.04595 = 0.03676 -0.00518 -0.00370 -0.01276 CL2 3 0.473280 0.401813 0.834062 11.00000 0.03437 0.04059 = 0.03127 -0.00571 -0.00409 -0.01077 O1 6 0.778288 0.370522 0.878847 11.00000 0.04008 0.05407 = 0.03000 -0.01353 -0.00884 -0.01614 N1 5 0.695451 0.177695 0.673771 11.00000 0.03225 0.02920 = 0.01715 0.00272 -0.01033 -0.01209 N2 5 0.685131 0.448349 0.548208 11.00000 0.03825 0.02407 = 0.02386 0.00137 -0.00931 -0.01072 N3 5 0.698625 0.606161 0.678367 11.00000 0.05410 0.02792 = 0.02847 -0.00564 -0.00365 -0.01354 C17 1 0.760845 0.452595 0.357844 11.00000 0.06241 0.04323 = 0.02111 0.00039 -0.00889 -0.01842 AFIX 137 H17A 2 0.673485 0.501035 0.342546 11.00000 -1.50000 H17B 2 0.803061 0.390859 0.310914 11.00000 -1.50000 H17C 2 0.822356 0.511902 0.346880 11.00000 -1.50000 AFIX 0 C16 1 0.735717 0.381952 0.470222 11.00000 0.03601 0.03464 = 0.02153 0.00083 -0.00767 -0.01443 C15 1 0.766775 0.247901 0.485483 11.00000 0.04265 0.03621 = 0.01910 -0.00697 -0.00407 -0.00989 AFIX 43 H15 2 0.813961 0.214523 0.423586 11.00000 -1.20000 AFIX 0 C14 1 0.739645 0.154048 0.577552 11.00000 0.04023 0.02415 = 0.02554 -0.00388 -0.01084 -0.00926 C13 1 0.767483 0.018690 0.558983 11.00000 0.07168 0.03273 = 0.02411 -0.01087 -0.01054 -0.01322 AFIX 137 H13A 2 0.864716 -0.019354 0.553756 11.00000 -1.50000 H13B 2 0.744483 0.020274 0.493454 11.00000 -1.50000 H13C 2 0.711304 -0.032641 0.617695 11.00000 -1.50000 AFIX 0 C18 1 0.643316 0.588966 0.517521 11.00000 0.05068 0.02968 = 0.03559 0.00442 -0.01408 -0.00757 AFIX 23 H18A 2 0.566837 0.608862 0.482782 11.00000 -1.20000 H18B 2 0.721176 0.624887 0.467051 11.00000 -1.20000 AFIX 0 C19 1 0.599093 0.648129 0.612763 11.00000 0.05241 0.02385 = 0.04419 -0.00356 -0.00443 -0.00340 AFIX 23 H19A 2 0.584942 0.742650 0.590445 11.00000 -1.20000 H19B 2 0.510110 0.625880 0.655471 11.00000 -1.20000 AFIX 0 C21 1 0.643636 0.668529 0.771654 11.00000 0.08547 0.02498 = 0.04730 -0.01740 -0.00568 -0.01209 AFIX 137 H21A 2 0.709157 0.641135 0.816030 11.00000 -1.50000 H21B 2 0.556143 0.643597 0.811968 11.00000 -1.50000 H21C 2 0.629363 0.761964 0.748449 11.00000 -1.50000 AFIX 0 C20 1 0.831767 0.643846 0.618275 11.00000 0.06264 0.03456 = 0.04466 -0.00541 -0.00361 -0.02588 AFIX 137 H20A 2 0.865961 0.607286 0.554396 11.00000 -1.50000 H20B 2 0.898291 0.611485 0.661789 11.00000 -1.50000 H20C 2 0.818815 0.737606 0.599028 11.00000 -1.50000 AFIX 0 C1 1 0.651998 0.075655 0.759949 11.00000 0.03459 0.01859 = 0.01670 -0.00407 -0.00374 -0.01086 C6 1 0.513869 0.060857 0.787588 11.00000 0.03443 0.02271 = 0.02303 -0.00433 -0.00697 -0.00827 C5 1 0.474461 -0.036091 0.871656 11.00000 0.04225 0.03132 = 0.02869 -0.00056 -0.00738 -0.01894 AFIX 43 H5 2 0.382678 -0.048849 0.890099 11.00000 -1.20000 AFIX 0 C4 1 0.564768 -0.114372 0.929130 11.00000 0.05375 0.03521 = 0.01415 0.00094 -0.00210 -0.02136 AFIX 43 H4 2 0.534701 -0.177906 0.987855 11.00000 -1.20000 AFIX 0 C3 1 0.699489 -0.098853 0.899903 11.00000 0.06138 0.02235 = 0.02228 -0.00203 -0.01677 -0.00829 AFIX 43 H3 2 0.762518 -0.154303 0.937915 11.00000 -1.20000 AFIX 0 C2 1 0.744814 -0.004700 0.816771 11.00000 0.03748 0.03264 = 0.02028 -0.00768 -0.00810 -0.01214 C7 1 0.895435 0.004047 0.788530 11.00000 0.03768 0.04152 = 0.03275 0.00296 -0.01530 -0.01016 AFIX 13 H7 2 0.910497 0.076006 0.726874 11.00000 -1.20000 AFIX 0 C8 1 0.935932 0.034059 0.877174 11.00000 0.05290 0.05120 = 0.06375 -0.01668 -0.02514 -0.01460 AFIX 137 H8A 2 0.877177 0.113800 0.896588 11.00000 -1.50000 H8B 2 1.031879 0.044126 0.854149 11.00000 -1.50000 H8C 2 0.924943 -0.036332 0.938140 11.00000 -1.50000 AFIX 0 C9 1 0.992648 -0.120100 0.756221 11.00000 0.05224 0.06325 = 0.04912 -0.02215 -0.01706 0.00194 AFIX 137 H9A 2 0.986036 -0.190895 0.817122 11.00000 -1.50000 H9B 2 1.087261 -0.106150 0.731191 11.00000 -1.50000 H9C 2 0.965936 -0.141524 0.699979 11.00000 -1.50000 AFIX 0 C10 1 0.409602 0.142492 0.727162 11.00000 0.03506 0.03884 = 0.03374 0.00008 -0.01378 -0.01199 AFIX 13 H10 2 0.449711 0.217042 0.680591 11.00000 -1.20000 AFIX 0 C12 1 0.381172 0.069391 0.657345 11.00000 0.07974 0.07809 = 0.05300 -0.01583 -0.04355 -0.00859 AFIX 137 H12A 2 0.464073 0.050202 0.601969 11.00000 -1.50000 H12B 2 0.306825 0.121619 0.625338 11.00000 -1.50000 H12C 2 0.354215 -0.010965 0.699540 11.00000 -1.50000 AFIX 0 C11 1 0.274911 0.196510 0.800578 11.00000 0.03506 0.05102 = 0.05189 -0.00611 -0.01110 -0.00984 AFIX 137 H11A 2 0.235136 0.125486 0.849501 11.00000 -1.50000 H11B 2 0.210304 0.247800 0.758701 11.00000 -1.50000 H11C 2 0.293477 0.250660 0.840307 11.00000 -1.50000 AFIX 0 C25 1 0.687300 0.347061 0.984814 11.00000 0.05234 0.09258 = 0.01827 -0.01240 -0.00902 -0.01232 AFIX 23 H25A 2 0.642733 0.273854 0.993900 11.00000 -1.20000 H25B 2 0.615368 0.423964 0.997479 11.00000 -1.20000 AFIX 0 C24 1 0.779445 0.317287 1.058281 11.00000 0.05746 0.07132 = 0.04120 -0.01585 -0.01780 -0.01320 AFIX 23 H24A 2 0.729493 0.344714 1.125798 11.00000 -1.20000 H24B 2 0.818984 0.224429 1.072309 11.00000 -1.20000 AFIX 0 C23 1 0.884606 0.391266 1.001131 11.00000 0.12179 0.13650 = 0.07142 0.00396 -0.05822 -0.07647 AFIX 23 H23A 2 0.971284 0.350585 1.022624 11.00000 -1.20000 H23B 2 0.856054 0.479270 1.016003 11.00000 -1.20000 AFIX 0 C22 1 0.904552 0.395558 0.887406 11.00000 0.05068 0.08812 = 0.04836 -0.01780 -0.01562 -0.03313 AFIX 23 H22A 2 0.920504 0.480850 0.845726 11.00000 -1.20000 H22B 2 0.983689 0.329335 0.862256 11.00000 -1.20000 AFIX 0 HKLF 4 REM 230608d_0m_a.res in P-1 REM wR2 = 0.1142, GooF = S = 1.080, Restrained GooF = 1.080 for all data REM R1 = 0.0430 for 4876 Fo > 4sig(Fo) and 0.0460 for all 5300 data REM 298 parameters refined using 0 restraints END WGHT 0.0733 0.0000 REM Highest difference peak 1.701, deepest hole -1.870, 1-sigma level 0.136 Q1 1 0.6887 0.3620 0.7807 11.00000 0.05 1.70 Q2 1 0.7542 0.3704 0.6433 11.00000 0.05 1.51 Q3 1 0.8490 0.3746 0.6604 11.00000 0.05 0.95 Q4 1 0.5790 0.3525 0.7587 11.00000 0.05 0.88 Q5 1 0.8643 0.3091 0.6453 11.00000 0.05 0.75 Q6 1 0.5903 0.4213 0.7934 11.00000 0.05 0.71 Q7 1 0.6387 0.3064 0.7066 11.00000 0.05 0.61 Q8 1 1.0102 0.3065 0.5839 11.00000 0.05 0.56 Q9 1 0.6828 0.5089 0.7893 11.00000 0.05 0.56 Q10 1 0.9378 0.3231 0.9668 11.00000 0.05 0.55 Q11 1 0.8300 -0.0943 0.8606 11.00000 0.05 0.55 ; _shelx_res_checksum 86613 _olex2_submission_special_instructions 'No special instructions were received' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Dy1 Dy 0.72023(2) 0.36457(2) 0.71579(2) 0.02386(14) Uani 1 1 d . . . . . Cl1 Cl 0.98455(13) 0.31528(13) 0.65101(11) 0.0391(3) Uani 1 1 d . . . . . Cl2 Cl 0.47328(13) 0.40181(13) 0.83406(11) 0.0358(3) Uani 1 1 d . . . . . O1 O 0.7783(4) 0.3705(4) 0.8788(3) 0.0390(9) Uani 1 1 d . . . . . N1 N 0.6955(4) 0.1777(4) 0.6738(3) 0.0254(9) Uani 1 1 d . . . . . N2 N 0.6851(4) 0.4483(4) 0.5482(3) 0.0286(9) Uani 1 1 d . . . . . N3 N 0.6986(5) 0.6062(4) 0.6784(4) 0.0372(10) Uani 1 1 d . . . . . C17 C 0.7608(7) 0.4526(6) 0.3578(4) 0.0422(14) Uani 1 1 d . . . . . H17A H 0.673485 0.501035 0.342546 0.063 Uiso 1 1 calc R U . . . H17B H 0.803061 0.390859 0.310914 0.063 Uiso 1 1 calc R U . . . H17C H 0.822356 0.511902 0.346880 0.063 Uiso 1 1 calc R U . . . C16 C 0.7357(5) 0.3820(5) 0.4702(4) 0.0303(11) Uani 1 1 d . . . . . C15 C 0.7668(5) 0.2479(5) 0.4855(4) 0.0327(11) Uani 1 1 d . . . . . H15 H 0.813961 0.214523 0.423586 0.039 Uiso 1 1 calc R U . . . C14 C 0.7396(5) 0.1540(5) 0.5776(4) 0.0290(11) Uani 1 1 d . . . . . C13 C 0.7675(7) 0.0187(5) 0.5590(5) 0.0415(14) Uani 1 1 d . . . . . H13A H 0.864716 -0.019354 0.553756 0.062 Uiso 1 1 calc R U . . . H13B H 0.744483 0.020274 0.493454 0.062 Uiso 1 1 calc R U . . . H13C H 0.711304 -0.032641 0.617695 0.062 Uiso 1 1 calc R U . . . C18 C 0.6433(6) 0.5890(5) 0.5175(5) 0.0399(13) Uani 1 1 d . . . . . H18A H 0.566837 0.608862 0.482782 0.048 Uiso 1 1 calc R U . . . H18B H 0.721176 0.624887 0.467051 0.048 Uiso 1 1 calc R U . . . C19 C 0.5991(6) 0.6481(5) 0.6128(5) 0.0431(14) Uani 1 1 d . . . . . H19A H 0.584942 0.742650 0.590445 0.052 Uiso 1 1 calc R U . . . H19B H 0.510110 0.625880 0.655471 0.052 Uiso 1 1 calc R U . . . C21 C 0.6436(8) 0.6685(6) 0.7717(5) 0.0527(17) Uani 1 1 d . . . . . H21A H 0.709157 0.641135 0.816030 0.079 Uiso 1 1 calc R U . . . H21B H 0.556143 0.643597 0.811968 0.079 Uiso 1 1 calc R U . . . H21C H 0.629363 0.761964 0.748449 0.079 Uiso 1 1 calc R U . . . C20 C 0.8318(7) 0.6438(6) 0.6183(5) 0.0467(15) Uani 1 1 d . . . . . H20A H 0.865961 0.607286 0.554396 0.070 Uiso 1 1 calc R U . . . H20B H 0.898291 0.611485 0.661789 0.070 Uiso 1 1 calc R U . . . H20C H 0.818815 0.737606 0.599028 0.070 Uiso 1 1 calc R U . . . C1 C 0.6520(5) 0.0757(4) 0.7599(4) 0.0226(10) Uani 1 1 d . . . . . C6 C 0.5139(5) 0.0609(4) 0.7876(4) 0.0262(10) Uani 1 1 d . . . . . C5 C 0.4745(6) -0.0361(5) 0.8717(4) 0.0331(12) Uani 1 1 d . . . . . H5 H 0.382678 -0.048849 0.890099 0.040 Uiso 1 1 calc R U . . . C4 C 0.5648(6) -0.1144(5) 0.9291(4) 0.0344(12) Uani 1 1 d . . . . . H4 H 0.534701 -0.177906 0.987855 0.041 Uiso 1 1 calc R U . . . C3 C 0.6995(6) -0.0989(5) 0.8999(4) 0.0343(12) Uani 1 1 d . . . . . H3 H 0.762518 -0.154303 0.937915 0.041 Uiso 1 1 calc R U . . . C2 C 0.7448(5) -0.0047(5) 0.8168(4) 0.0284(11) Uani 1 1 d . . . . . C7 C 0.8954(6) 0.0040(5) 0.7885(5) 0.0373(13) Uani 1 1 d . . . . . H7 H 0.910497 0.076006 0.726874 0.045 Uiso 1 1 calc R U . . . C8 C 0.9359(7) 0.0341(7) 0.8772(6) 0.0516(16) Uani 1 1 d . . . . . H8A H 0.877177 0.113800 0.896588 0.077 Uiso 1 1 calc R U . . . H8B H 1.031879 0.044126 0.854149 0.077 Uiso 1 1 calc R U . . . H8C H 0.924943 -0.036332 0.938140 0.077 Uiso 1 1 calc R U . . . C9 C 0.9926(7) -0.1201(7) 0.7562(6) 0.0542(17) Uani 1 1 d . . . . . H9A H 0.986036 -0.190895 0.817122 0.081 Uiso 1 1 calc R U . . . H9B H 1.087261 -0.106150 0.731191 0.081 Uiso 1 1 calc R U . . . H9C H 0.965936 -0.141524 0.699979 0.081 Uiso 1 1 calc R U . . . C10 C 0.4096(5) 0.1425(5) 0.7272(4) 0.0351(12) Uani 1 1 d . . . . . H10 H 0.449711 0.217042 0.680591 0.042 Uiso 1 1 calc R U . . . C12 C 0.3812(9) 0.0694(8) 0.6573(6) 0.065(2) Uani 1 1 d . . . . . H12A H 0.464073 0.050202 0.601969 0.097 Uiso 1 1 calc R U . . . H12B H 0.306825 0.121619 0.625338 0.097 Uiso 1 1 calc R U . . . H12C H 0.354215 -0.010965 0.699540 0.097 Uiso 1 1 calc R U . . . C11 C 0.2749(6) 0.1965(6) 0.8006(6) 0.0463(15) Uani 1 1 d . . . . . H11A H 0.235136 0.125486 0.849501 0.069 Uiso 1 1 calc R U . . . H11B H 0.210304 0.247800 0.758701 0.069 Uiso 1 1 calc R U . . . H11C H 0.293477 0.250660 0.840307 0.069 Uiso 1 1 calc R U . . . C25 C 0.6873(7) 0.3471(8) 0.9848(5) 0.0543(18) Uani 1 1 d . . . . . H25A H 0.642733 0.273854 0.993900 0.065 Uiso 1 1 calc R U . . . H25B H 0.615368 0.423964 0.997479 0.065 Uiso 1 1 calc R U . . . C24 C 0.7794(7) 0.3173(7) 1.0583(6) 0.0543(17) Uani 1 1 d . . . . . H24A H 0.729493 0.344714 1.125798 0.065 Uiso 1 1 calc R U . . . H24B H 0.818984 0.224429 1.072309 0.065 Uiso 1 1 calc R U . . . C23 C 0.8846(12) 0.3913(12) 1.0011(7) 0.097(4) Uani 1 1 d . . . . . H23A H 0.971284 0.350585 1.022624 0.116 Uiso 1 1 calc R U . . . H23B H 0.856054 0.479270 1.016003 0.116 Uiso 1 1 calc R U . . . C22 C 0.9046(7) 0.3956(8) 0.8874(6) 0.0570(18) Uani 1 1 d . . . . . H22A H 0.920504 0.480850 0.845726 0.068 Uiso 1 1 calc R U . . . H22B H 0.983689 0.329335 0.862256 0.068 Uiso 1 1 calc R U . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Dy1 0.03091(18) 0.02325(18) 0.02004(18) -0.00422(10) -0.00557(11) -0.01060(10) Cl1 0.0327(6) 0.0459(7) 0.0368(8) -0.0052(6) -0.0037(5) -0.0128(5) Cl2 0.0344(6) 0.0406(7) 0.0313(7) -0.0057(5) -0.0041(5) -0.0108(5) O1 0.040(2) 0.054(2) 0.030(2) -0.0135(18) -0.0088(17) -0.0161(18) N1 0.032(2) 0.029(2) 0.017(2) 0.0027(16) -0.0103(17) -0.0121(17) N2 0.038(2) 0.024(2) 0.024(2) 0.0014(17) -0.0093(19) -0.0107(17) N3 0.054(3) 0.028(2) 0.028(3) -0.0056(19) -0.004(2) -0.014(2) C17 0.062(4) 0.043(3) 0.021(3) 0.000(2) -0.009(3) -0.018(3) C16 0.036(3) 0.035(3) 0.022(3) 0.001(2) -0.008(2) -0.014(2) C15 0.043(3) 0.036(3) 0.019(3) -0.007(2) -0.004(2) -0.010(2) C14 0.040(3) 0.024(2) 0.026(3) -0.004(2) -0.011(2) -0.009(2) C13 0.072(4) 0.033(3) 0.024(3) -0.011(2) -0.011(3) -0.013(3) C18 0.051(3) 0.030(3) 0.036(3) 0.004(2) -0.014(3) -0.008(2) C19 0.052(3) 0.024(3) 0.044(4) -0.004(2) -0.004(3) -0.003(2) C21 0.085(5) 0.025(3) 0.047(4) -0.017(3) -0.006(4) -0.012(3) C20 0.063(4) 0.035(3) 0.045(4) -0.005(3) -0.004(3) -0.026(3) C1 0.035(2) 0.019(2) 0.017(2) -0.0041(18) -0.004(2) -0.0109(19) C6 0.034(2) 0.023(2) 0.023(3) -0.0043(19) -0.007(2) -0.0083(19) C5 0.042(3) 0.031(3) 0.029(3) -0.001(2) -0.007(2) -0.019(2) C4 0.054(3) 0.035(3) 0.014(2) 0.001(2) -0.002(2) -0.021(2) C3 0.061(3) 0.022(2) 0.022(3) -0.002(2) -0.017(3) -0.008(2) C2 0.037(3) 0.033(3) 0.020(3) -0.008(2) -0.008(2) -0.012(2) C7 0.038(3) 0.042(3) 0.033(3) 0.003(2) -0.015(2) -0.010(2) C8 0.053(4) 0.051(4) 0.064(5) -0.017(3) -0.025(3) -0.015(3) C9 0.052(4) 0.063(4) 0.049(4) -0.022(3) -0.017(3) 0.002(3) C10 0.035(3) 0.039(3) 0.034(3) 0.000(2) -0.014(2) -0.012(2) C12 0.080(5) 0.078(5) 0.053(5) -0.016(4) -0.044(4) -0.009(4) C11 0.035(3) 0.051(4) 0.052(4) -0.006(3) -0.011(3) -0.010(3) C25 0.052(4) 0.093(5) 0.018(3) -0.012(3) -0.009(3) -0.012(4) C24 0.057(4) 0.071(5) 0.041(4) -0.016(3) -0.018(3) -0.013(3) C23 0.122(8) 0.136(9) 0.071(6) 0.004(6) -0.058(6) -0.076(7) C22 0.051(4) 0.088(5) 0.048(4) -0.018(4) -0.016(3) -0.033(4) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0137 0.0067 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.3281 0.5435 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Dy Dy -5.9987 12.4498 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0241 0.0134 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0389 0.0241 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Cl1 Dy1 Cl2 162.92(5) . . ? O1 Dy1 Cl1 81.50(9) . . ? O1 Dy1 Cl2 81.74(9) . . ? O1 Dy1 N3 84.95(15) . . ? N1 Dy1 Cl1 93.25(10) . . ? N1 Dy1 Cl2 93.47(11) . . ? N1 Dy1 O1 124.32(13) . . ? N1 Dy1 N3 150.47(15) . . ? N2 Dy1 Cl1 94.19(11) . . ? N2 Dy1 Cl2 102.41(11) . . ? N2 Dy1 O1 154.88(14) . . ? N2 Dy1 N1 80.48(14) . . ? N2 Dy1 N3 70.74(15) . . ? N3 Dy1 Cl1 95.27(12) . . ? N3 Dy1 Cl2 86.52(11) . . ? C25 O1 Dy1 124.3(3) . . ? C22 O1 Dy1 126.9(4) . . ? C22 O1 C25 108.8(5) . . ? C14 N1 Dy1 122.5(3) . . ? C14 N1 C1 118.7(4) . . ? C1 N1 Dy1 117.9(3) . . ? C16 N2 Dy1 122.3(3) . . ? C16 N2 C18 116.8(4) . . ? C18 N2 Dy1 118.4(3) . . ? C19 N3 Dy1 101.5(3) . . ? C19 N3 C21 108.8(5) . . ? C19 N3 C20 110.5(5) . . ? C21 N3 Dy1 115.8(3) . . ? C20 N3 Dy1 111.1(4) . . ? C20 N3 C21 109.0(5) . . ? H17A C17 H17B 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? N2 C16 C17 119.6(5) . . ? N2 C16 C15 124.2(5) . . ? C15 C16 C17 116.2(5) . . ? C16 C15 H15 114.6 . . ? C16 C15 C14 130.7(5) . . ? C14 C15 H15 114.6 . . ? N1 C14 C15 124.7(5) . . ? N1 C14 C13 120.7(4) . . ? C15 C14 C13 114.7(5) . . ? C14 C13 H13A 109.5 . . ? C14 C13 H13B 109.5 . . ? C14 C13 H13C 109.5 . . ? H13A C13 H13B 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? N2 C18 H18A 109.7 . . ? N2 C18 H18B 109.7 . . ? N2 C18 C19 109.6(4) . . ? H18A C18 H18B 108.2 . . ? C19 C18 H18A 109.7 . . ? C19 C18 H18B 109.7 . . ? N3 C19 C18 113.2(5) . . ? N3 C19 H19A 108.9 . . ? N3 C19 H19B 108.9 . . ? C18 C19 H19A 108.9 . . ? C18 C19 H19B 108.9 . . ? H19A C19 H19B 107.8 . . ? N3 C21 H21A 109.5 . . ? N3 C21 H21B 109.5 . . ? N3 C21 H21C 109.5 . . ? H21A C21 H21B 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? N3 C20 H20A 109.5 . . ? N3 C20 H20B 109.5 . . ? N3 C20 H20C 109.5 . . ? H20A C20 H20B 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C6 C1 N1 119.1(4) . . ? C2 C1 N1 120.4(4) . . ? C2 C1 C6 120.5(4) . . ? C1 C6 C10 122.9(4) . . ? C5 C6 C1 117.9(4) . . ? C5 C6 C10 119.2(4) . . ? C6 C5 H5 119.0 . . ? C4 C5 C6 122.0(5) . . ? C4 C5 H5 119.0 . . ? C5 C4 H4 120.5 . . ? C5 C4 C3 119.0(5) . . ? C3 C4 H4 120.5 . . ? C4 C3 H3 119.2 . . ? C4 C3 C2 121.6(5) . . ? C2 C3 H3 119.2 . . ? C1 C2 C7 122.8(4) . . ? C3 C2 C1 119.0(5) . . ? C3 C2 C7 118.2(5) . . ? C2 C7 H7 107.6 . . ? C2 C7 C9 112.7(5) . . ? C8 C7 C2 112.2(5) . . ? C8 C7 H7 107.6 . . ? C8 C7 C9 108.8(5) . . ? C9 C7 H7 107.6 . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8B 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9B 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C6 C10 H10 107.5 . . ? C6 C10 C11 112.0(5) . . ? C12 C10 C6 111.7(5) . . ? C12 C10 H10 107.5 . . ? C12 C10 C11 110.3(5) . . ? C11 C10 H10 107.5 . . ? C10 C12 H12A 109.5 . . ? C10 C12 H12B 109.5 . . ? C10 C12 H12C 109.5 . . ? H12A C12 H12B 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11B 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? O1 C25 H25A 110.8 . . ? O1 C25 H25B 110.8 . . ? O1 C25 C24 104.9(5) . . ? H25A C25 H25B 108.8 . . ? C24 C25 H25A 110.8 . . ? C24 C25 H25B 110.8 . . ? C25 C24 H24A 111.2 . . ? C25 C24 H24B 111.2 . . ? H24A C24 H24B 109.1 . . ? C23 C24 C25 102.9(6) . . ? C23 C24 H24A 111.2 . . ? C23 C24 H24B 111.2 . . ? C24 C23 H23A 110.2 . . ? C24 C23 H23B 110.2 . . ? C24 C23 C22 107.7(6) . . ? H23A C23 H23B 108.5 . . ? C22 C23 H23A 110.2 . . ? C22 C23 H23B 110.2 . . ? O1 C22 C23 104.9(6) . . ? O1 C22 H22A 110.8 . . ? O1 C22 H22B 110.8 . . ? C23 C22 H22A 110.8 . . ? C23 C22 H22B 110.8 . . ? H22A C22 H22B 108.8 . . ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Dy1 Cl1 2.5864(13) . ? Dy1 Cl2 2.5925(13) . ? Dy1 O1 2.475(4) . ? Dy1 N1 2.354(4) . ? Dy1 N2 2.324(4) . ? Dy1 N3 2.535(4) . ? O1 C25 1.472(7) . ? O1 C22 1.448(7) . ? N1 C14 1.319(7) . ? N1 C1 1.453(6) . ? N2 C16 1.340(7) . ? N2 C18 1.479(7) . ? N3 C19 1.471(8) . ? N3 C21 1.487(8) . ? N3 C20 1.487(7) . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C17 C16 1.505(7) . ? C16 C15 1.399(8) . ? C15 H15 0.9500 . ? C15 C14 1.411(7) . ? C14 C13 1.511(7) . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C18 C19 1.492(9) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C1 C6 1.414(7) . ? C1 C2 1.401(7) . ? C6 C5 1.391(7) . ? C6 C10 1.518(7) . ? C5 H5 0.9500 . ? C5 C4 1.381(8) . ? C4 H4 0.9500 . ? C4 C3 1.382(8) . ? C3 H3 0.9500 . ? C3 C2 1.381(7) . ? C2 C7 1.521(7) . ? C7 H7 1.0000 . ? C7 C8 1.515(8) . ? C7 C9 1.554(9) . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10 1.0000 . ? C10 C12 1.514(9) . ? C10 C11 1.538(9) . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C25 C24 1.500(9) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C24 C23 1.446(11) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C23 C22 1.484(11) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Dy1 O1 C25 C24 161.7(4) . . . . ? Dy1 O1 C22 C23 178.6(6) . . . . ? Dy1 N1 C14 C15 -20.3(7) . . . . ? Dy1 N1 C14 C13 158.6(4) . . . . ? Dy1 N1 C1 C6 101.8(4) . . . . ? Dy1 N1 C1 C2 -76.4(5) . . . . ? Dy1 N2 C16 C17 -155.4(4) . . . . ? Dy1 N2 C16 C15 25.3(7) . . . . ? Dy1 N2 C18 C19 -13.6(6) . . . . ? Dy1 N3 C19 C18 -56.4(5) . . . . ? O1 C25 C24 C23 30.6(9) . . . . ? N1 C1 C6 C5 -178.8(5) . . . . ? N1 C1 C6 C10 3.5(7) . . . . ? N1 C1 C2 C3 178.4(5) . . . . ? N1 C1 C2 C7 -3.8(7) . . . . ? N2 C16 C15 C14 8.6(9) . . . . ? N2 C18 C19 N3 50.1(6) . . . . ? C17 C16 C15 C14 -170.8(5) . . . . ? C16 N2 C18 C19 -176.0(5) . . . . ? C16 C15 C14 N1 -11.3(9) . . . . ? C16 C15 C14 C13 169.7(6) . . . . ? C14 N1 C1 C6 -88.8(6) . . . . ? C14 N1 C1 C2 93.0(6) . . . . ? C18 N2 C16 C17 6.2(7) . . . . ? C18 N2 C16 C15 -173.1(5) . . . . ? C21 N3 C19 C18 -178.9(5) . . . . ? C20 N3 C19 C18 61.5(6) . . . . ? C1 N1 C14 C15 170.8(5) . . . . ? C1 N1 C14 C13 -10.3(7) . . . . ? C1 C6 C5 C4 1.7(8) . . . . ? C1 C6 C10 C12 103.9(6) . . . . ? C1 C6 C10 C11 -131.9(5) . . . . ? C1 C2 C7 C8 119.9(6) . . . . ? C1 C2 C7 C9 -116.9(6) . . . . ? C6 C1 C2 C3 0.2(7) . . . . ? C6 C1 C2 C7 178.0(5) . . . . ? C6 C5 C4 C3 -2.3(8) . . . . ? C5 C6 C10 C12 -73.8(7) . . . . ? C5 C6 C10 C11 50.5(7) . . . . ? C5 C4 C3 C2 2.0(8) . . . . ? C4 C3 C2 C1 -0.9(8) . . . . ? C4 C3 C2 C7 -178.8(5) . . . . ? C3 C2 C7 C8 -62.3(7) . . . . ? C3 C2 C7 C9 60.9(7) . . . . ? C2 C1 C6 C5 -0.6(7) . . . . ? C2 C1 C6 C10 -178.2(5) . . . . ? C10 C6 C5 C4 179.4(5) . . . . ? C25 O1 C22 C23 -2.1(9) . . . . ? C25 C24 C23 C22 -32.7(11) . . . . ? C24 C23 C22 O1 22.2(11) . . . . ? C22 O1 C25 C24 -17.7(8) . . . . ?